TRNG I HC CNG NGHIP TP.

HCM KHOA CNG NGH HA HC

TIU LUN MN PHN TCH CNG NGHIP

PHN TCH CC CH TIU HA HC TRONG CAO SU

GVHD: SVTH:

Ths. H VN TI TRN CM BA NGUYN THANH NGC HNH L TH MINH NHT HAN QUYN TRN KIM TRINH CHU TH ANH TRC 11301011 11299521 11310461 11331331 11245741 11316211

Thnh ph H Ch Minh, ngy 11 thng 03 nm 2012

Chng 1 TNG QUAN V CAO SU

1.1. Gii thiu v cao su Cao su t nhin hay cao su thin nhin l loi vt liu c sn xut t m cy cao su (Hevea brasiliensis) ca h i Kch (Euphorbiaceae). Nhng ngi dn Nam M l nhng ngi u tin pht hin v s dng cao su t nhin th k 16. Henry Wickham hi hng ngn ht Brasil vo nm 1876 v mang nhng ht n Kew Gardens (Anh) cho ny mm. Cc cy con c gi n Colombo, Indonesia, v Singapore. Tuy nhin, vic s dng cao su tr nn ph bin ch khi qu trnh lu ha cao su c cc nh ha hc, tm ra vo nm 1839. Khi , cao su t nhin chuyn t trng thi chy nht sang trng thi n hi cao. M cao su thin nhin l dng nh tng trong nc ca cc ht cao su vi hm lng phn kh t 28%-40%. Kch thc ht cao su rt nh, c khong 0,053 v c hnh qu trng g. Trong 1 gam m cao su vi hm lng phn kh 40% c 5000 ht vi ng knh trung bnh 0,26, tt c cc ht ny u trng thi chuyn ng Browner. 1.2. Cu to ha hc V mt ha hc, cao su thin nhin l polyisopren - polyme ca isopren

Mch i phn t ca cao su thin nhin c hnh thnh t cc mt xch isopren ng phn cis lin kt vi nhau v tr 1,4.

Ngoi ng phn cis 1,4, trong cao su thin nhin cn c khong 2% mt xch lin kt vi nhau v tr 3,4. C cu to tng t vi cao su thin nhin, nha cy Gutapertra c hnh thnh t polyme ca isopren ng phn trans 1,4. 1.3. Tnh cht vt l nhit thp, cao su thin nhin c cu trc tinh th . Cao su thin nhin kt tinh vi vn tc nhanh nht -25C. CSTN tinh th nng chy 40C. Khi lng ring 913 kg/cm. Cao su thin nhin tan tt trong cc dung mi hu c mch thng, mch vng v CCl4. Tuy nhin, cao su thin nhin khng tan trong ru v xeton.

CHNG 2 PHN TCH CC CH TIU HA HC TRONG CAO SU

2.1. Phn tch cc ch tiu ha hc trong cao su thin nhin 2.1.1. Phn tch hm lng cht bay hi 2.1.1.1. Phm vi p dng C hai phng php xc nh m v hm lng cht bay hi trong cao su th l phng php cn nng v phng php l sy. Cc phng php ny cng c th c p dng cho cc loi cao su khc, nhng khi cn phi chng minh rng s thay i khi lng ch do mt cc cht bay hi gc m khng phi do phn hy cao su. Phng php cn nng khng p dng c i vi cao su thin nhin v cao su tng hp isoprene hay i cao su qu kh cn nng hoc cao su dng bt hay dng mnh. Hai phng php th ny khng cho kt qu ng nht. do vy, trong trng hp tranh chp, phng php l sy l phng php trng ti. 2.1.1.2. Nguyn tc a. Phng php cn nng Phn mu th c cn thnh tm trn my cn lm nng cho n khi tt c cc cht bay hi bay ht. Khi lng b mt trong lc cn c tnh ton v biu th hm lng cht bay hi. b. Phng php l sy Nu mu khng phi dng bt, s dng my cn phng th nghim ng nht mt phn mu th. Mt phn mu th c ly t phn ng nht hoc ly trc tip t cao su nu mu dng bt, c dn thnh tm v lm kh trong l nung n khi lng khng i. Hm lng cht bay hi c tnh theo khi lng b mt trong qu trnh th, cng vi khi lng b mt trong lc ng nht phn mu th. 2.1.1.3. Thit b _ My cn trn (dng cho phng php cn nng).

_ L sy c lp thit b thng gi, tt nht l loi tun hon khng kh, c kh nng duy tr nhit 1050C 50C (dng cho phng php l sy). 2.1.1.4. Cch tin hnh a. Phng php cn nng _ Cn thnh tm mt ming mu th khong 250 g. Cn chnh xc n 0.1 g trc v sau khi ng nht (ghi khi lng m1 v m2 tng ng). _ Dng mnh ch, iu chnh khe h trc cn n 0.25 mm 0.05 mm. Gi nhit b mt ca trc 1050C 50C. _ Mt phn mu th cn (khi lng m3) c cn li trn my cn trong 4 pht. Khng c cho phn mu th b cn thnh ai v cn thn chng tht thot cao su. Cn mu th chnh xc n 0.1 g. Cho phn mu th qua my cn thm 2 pht v cn li. Nu khi lng sau khi cn 4 pht v 6 pht nh hn 0.1 g, tnh hm lng cht bay hi; nu chnh lch khng t yu cu trn, tip tc cho phn mu th qua my cn 2 pht na cho n khi khi lng khng gim qu 0.1 g gia cc ln cn lin tip (khi lng cui cng m4). Trc mi ln cn, lm ngui cao su n nhit phng trong bnh ht m. _ Nu cao su b bong ra tng mng hay tr thnh keo dnh trn trc my cn, gy kh khn cho vic cn hoc khng th cn c khi s dng phng php l sy. b. Phng php l sy Trong trng hp cao su thin nhin, tin hnh nh sau: _ Nu cao su khng dng bt, chn mt phn mu th khong 600g v ng nht. Cn phn mu chnh xc n 0.1 g trc v sau khi ng nht (ghi khi lng m5 v m6 tng ng). ngui n nhit phng trc khi cn ln cui. _ Chn mu th khong 10 g t phn mu th ng nht v cn chnh xc n 1 mg (ghi khi lng m1). _ t my cn nhit 700C 50C, cho phn mu th qua gia cc trc v cn hai ln thnh tm c chiu dy nh hn 2 mm.

_ Trong trng hp cao su dng bt, chn ngu nhin mt phn mu th khong 10 g v t ln trn mt knh ng h hoc mt khay nhm d cn. Cn chnh xc n 1mg (ghi khi lng m7). Trong trng hp cao su tng hp, tin hnh nh sau: _ Nu mu khng dng bt, chn mt phn mu th khong 250 g v ng nht. Cn chnh xc n 0.1g trc v sau khi ng nht (ghi khi lng m5 v m6 tng ng). _ t my cn nhit 700C 50C, v cn 10 g, chnh xc n 1mg (ghi khi lng m7). _ Nu khng th c tm mu ny, ly 10 g mu th t phn mu th ng nht v ct n bng tay thnh nhng hnh khi nh vi cc cnh di xp x 2 mm. t cc hnh khi ln mt knh ng h hay khay nhm d cn. Cn chnh xc n 1 mg (ghi khi lng m7). _ Trong trng hp cao su dng bt, chn ngu nhin mt phn mu th khong 10 g v t ln mt knh ng h hay khay nhm d cn. Cn chnh xc n 1 mg (ghi khi lng m7). _ t phn mu th vo trong l sy ) v sy trong 1 gi, duy tr nhit 700C 50C vi qut tun hon khng kh. Sp xp cao su sao cho din tch b mt tip xc vi kh nng l ln nht. ngui trong bnh ht m v cn. Lp li qu trnh sy trong cc khong thi gian 30 pht tip sau cho n khi khi lng gim khng ln hn 1 mg gia cc ln cn lin tip (ghi khi lng cui cng m8). 2.1.1.5. Cng thc tnh a. Phng php cn nng Hm lng cht bay hi (X) tnh bng phn trm khi lng, theo cng thc: X = [1 (m2 m4)/(m1m3)] 100 Trong : m1 l khi lng ca phn mu th trc khi ng nht (g) m2 l khi lng ca phn mu th sau khi ng nht (g) m3 l khi lng ca phn mu th trc khi cn (g)

m4 l khi lng ca phn mu th sau khi cn (g) b. Phng php l sy Nu phn mu th c ly t mu th ng nht, hm lng cht bay hi (X), c tnh bng phn trm, theo cng thc: X = [(m5 m6)/m5 (m7 m8/m7] 100

Trong : m5 l khi lng ca mu th trc khi ng nht (g) m6 l khi lng ca mu th sau khi ng nht (g) m7 l khi lng ca phn mu th ly t mu th (g) m8 l khi lng ca phn mu th sau khi sy kh trong l (g) Nu phn mu th c ly trc tip t mu dng bt, hm lng cht bay hi (X), tnh bng phn trm theo khi lng, theo cng thc: X = [(m7 m8)/m7] 100 Trong : m7 l khi lng ca phn mu th ly t mu th (g) m8 l khi lng ca phn mu th sau khi sy kh trong l (g) 2.1.2. Phn tch hm lng tro 2.1.2.1. Phm vi p dng Xc nh hm lng tro di vi cao su thin nhin th, cao su hn hp v cao su lu ha. Phng php ny cng p dng cho cao su th thin nhin, hn hp hoc lu ha h M, N, O, R v U. Phng php A khng p dng xc nh hm lng tro ca cao su hn hp hoc lu ha cha clo, brom hoc iot. Phng php B p dng xc nh hm lng tro ca cao su hn hp hoc lu ha cha clo, brom hoc iot. Khng s dng phng php ny cho cao su khng pha trn.

Hn hp liti v fluo c th phn ng vi chn nung silic to ra hn hp bay hi, cho kt qu hm lng tro thp. Chn nung platin c s dng ha tro cao su cha flo v cao su liti- polime ha. 2.1.2.2. Nguyn tc a. Phng php A Mt mu th cn c nung trong chn nung trn n kh. Sau khi bay hi, cc sn phm phn hy, chn nung c chuyn sang l nung, chn nung c nung cho n khi ha tro hon ton v thu c khi lng khng i. b. Phng php B Mt lng mu th c nung trong chn c axit sunfuric, trc tin nung trn n kh v sau trong l nung cho n khi ha tro hon ton v thu c khi lng khng i. 2.1.2.3. Thuc th Axit sunfuric m c (ch cho phng php B), TKPT, d= 1.84 g/cm3. 2.1.2.4. Thit b _ Chn nung, bng s, silic hoc platin vi dung tch khong 50 cm3. i vi cao su th tng hp, phi s dng chn nung c dung tch ti thiu 25 cm3 trn mt gam mu th. _ Tm cch nhit, chu nhit, c din tch 100 mm2 v chiu dy khong 5 mm c l hng tm ph hp vi chn nung. Khong 2/3 chn nung s nh ra khi tm cch nhit. _ n Busen hoc loi tng t n kh. _ L nung, gn mt ng khi kim sot dng khng kh trong l. Thit b iu chnh nhit gi cho nhit 550oC 25oC. 2.1.2.5. Chun b mu th _ Phn mu th ca cao su th thin nhin dc ct t mu ng nht chun b. Phn mu th ca cao su th tng hp c ct ra t cao su kh thu c sau khi tin hnh xc nh hm lng cht bay hi. _ Phn mu th ca cao su hn hp c chia nh bng tay.

_ Phn mu th ca cao su lu ha c cn thnh t trn my cn hoc bp vn hoc chia nh bng tay. 2.1.2.6. Cch tin hnh a. Phng php A Chn nung rng v sch vi kch c thch hp c nung khong 30 pht trong l nung, gi nhit ti 550oC 25oC, ngui n nhit mi trng trong bnh ht m v cn chnh xc n 0.1 mg. Ly khong 5 g mu th cao su th, 1 g n 5 g cao su hn hp hoc lu ha ty theo khi lng tro d kin xc nh, cn chnh xc n 0.1mg. t phn mu th cn vo chn nung gn vo l trong tm chu nhit, cch nhit. Nung nh chn nung trn n kh trong t ht cho thng thong thch hp, cn thn cao su khng b bt la. Nu bt k mu no b mt do bn ra hoc si bt, lp li qu trnh trn vi mt mu th mi. Khi cao su b phn hy n khi lng than ha, t t tng nhit n kh cho n khi cht phn hy bay hi b ui ht v thu c cn cacbon kh. Chuyn chn nung v cc cht trong chn vo l nung, gi nhit 550oC 25oC, m ca l mt cch nh nhng cung cp y khng kh cho s oxi ha cacbon. Tip tc nung cho n khi cacbon b oxi ha hon ton v thu c tro sch. Ly chn nung v cc cht trong ra khi l nung, ngui n nhit mi trng trong bnh ht m v cn li chnh xc n 0.1 mg. Khi lng ny s khc khi lng lc trc hn 1 mg trong trng hp cao su th hoc hn 1% tng i so vi lng tro ca cao su hn hp v lu ha. Nu yu cu ny khng c p ng, lp li cc qu trnh nung, ngui v cn cho dn khi chnh lch gia hai ln cn lin tip p ng yu cu trn. b. Phng php B Chn nung rng v sch vi kch c thch hp c nung khong 30 pht trong l nung, gi nhit ti 550oC 25oC, ngui n nhit mi trng trong bnh ht m v cn chnh xc n 0.1 mg. Ly khong 1 g n 5 g cao su hn hp hoc lu ha v cn chnh xc n 0.1 mg. Cho mu th vo chn nung v rt khong 3.5 cm3 axit sunfuric m c ln mu sao cho cao su c thm t hon ton. chn nung v cc cht c trong chn vo l trong tm chu

nhit, cch nhit v nung nh chn nung trn n kh trong t ht cho thng thong thch hp. Nu trong lc phn ng bt u, hn hp n ra qu nhiu, gim bt la trnh tht thot mu. Khi phn ng tr nn du hn, tng nhit n kh cho n khi axit sunfuric tha bay hi v mt lng cn cacbon c gi li. Chuyn chn nung v cc cht trong chn vo l nung gi nhit 950oC 25oC, v nung khong 1 gi cho n khi cacbon b oxi ha hon ton v thu c tro sch. Ly chn nung v cc cht trong chn ra khi l, ngui n nhit mi trng trong bnh ht m v cn chnh xc n 0.1 mg. Sau li nung chn nung v cc cht trong chn khong 30 pht trong l nung, gi nhit 950oC 25oC, ngui n nhit mi trng trong bnh ht m v cn li chnh xc n 0.1 mg. Nu khi lng ny chnh lch vi khi lng lc trc hn 1% tng i so vi lng tro, lp li cc qu trnh nung, ngui v cn cho dn khi chnh lch gia hai ln cn lin tip nh hn 1% tng i so vi lng tro. 2.1.2.7. Cng thc tnh Hm lng tro (X) tnh bng phn trm khi lng, theo cng thc: X = [(m2 - m1) / m0 ]x 100 Trong : m0 khi lng ca phn mu th (g) m1 khi lng ca chn nung rng (g) m2 khi lng ca chn nung v tro (g) 2.1.3. Phn tch hm lng nit 2.1.3.1. Phm vi p dng Xc nh hm lng nit trong cao su thin nhin th v latex cao su thin nhin bng phng php Kendan. 2.1.3.2. Nguyn tc Mt lng mu bit c phn hy bng hn hp axit sunfurric, kali sunfat v lng xc tc ng sunfat, selen hoc natri selenat, do vy bin i cc

hp cht nit thnh amoni hydro sunfat, t amoniac c chng ct sau khi to thnh hn hp kim. Amoniac chng ct c hp th: _ Trong dung dch axit sunfuric th tch chun sau l chun axit tha bng dung dch baz th tch chun _ Trong dung dch axit boric sau l chun bng dung dch axit th tch chun (v axit boric l mt axit yu nn n khng nh hng n cht ch th c s dng trong php chun ny). 2.1.3.3. Thuc th Trong sut qu trnh phn tch, tr khi c quy nh khc, ch s dng thuc th c TKPT, nc ct hoc nc c tinh khit tng ng. a. Hn hp cht xc tc Chun b hn hp trn k c chia nh gm: _ 30 phn, theo khi lng, kali sunfat (k2SO4). _ 4 phn, theo khi lng, ng sunfat ngm 5 phn t nc (CuSO4.5H2O). _ 1 phn, theo khi lng, bt Selen, hoc 2 phn theo khi lng, natri selenat ngm 10 phn t nc (Na2SeO4.10 H2O). b. Dung dch cht xc tc Ha tan bng cch un nng: _ 110 g kali sunfat khan _ 14.7 g ng sunfat ngm 5 phn t nc. _ 3,7 g Selen hoc 7,49 g natri selenat. Trong 600 cm3 axit sunfuric. _ Axit sunfuric, d= 1,84 g/cm3. _ Axit sunfuric, dung dch th tch chun, c= 0,05 mol/l. _ Natri hydroxit, dung dch th tch chun, c= 0,1 mol/l. _ Natri hydroxit, dung dch, c= 10 mol/l. Ha tan trong 400 g natri hydroxit rn trong 600 cm3 nc. _ Axit boric, dung dch, c= 0,17 mol/l.

Ha tan 40 g axit boric rn trong 1l nc, nu cn thit th trong nc m, v lm ngui n nhit phng. c. Dung dch hn hp ch th Ha tan 0,1 g metyl v 0,05 g metylen xanh trong 100 cm3 etanol 96% (V/V). 2.1.3.4. Thit b Cc thit b thng thng trong phng th nghim v thit b Kendan, vi bnh phn gii c dung tch 800cm3. 2.1.3.5. Ly mu v chun b phn mu th xc nh hm lng nit trong cao su rn th, ct mt mu th t mu ng nht. xc nh hm lng nit trong latex, phn mu i din t latex hn hp cha khang 2 g cht rn tng phi c lm kh n khi lng khng i. 2.1.3.6. Cch tin hnh _ Cn khang 2 g cao su hoc latex kh chnh xc n 0,5 mg, ct thnh nhng ming nh v cho vo bnh phn gii. Thm khang 13 g hn hp cht xc tc v 60 cm3 axit sunfuric hoc 65 cm3 dung dch cht xc tc. Trn cc cht trong bnh bng cch lc xoay trn, au un si nh cho n khi ha tan han tan. Tip tc un si thm mt gi. _ ngui bnh phn gii v cc cht trong n nhit phng, cn thn thm vo 200 cm3 nc v trn bng cch lc xoay trn. _ t bnh cha dung dch hp th vo v tr ni vi thet b chng ct, sau thm t t 150 cm3 dung dch natri hydroxit vo bnh phn gii bng mt phu nh git. _ Thc hin vic hp th v chun amoniac c gii phng theo mt trng hai cch sau. Gi bnh cha nhit di 30oC trnh s tht that amoniac. + Hp th bng axit sunfuric: Dng pipet thm 75 cm3 nc v 25 cm3 dung dch axit sunfuric chun vo bnh cha ca thit b chng ct cng vi hai git dung dch cht ch th hn hp.

t bnh cha sao cho phn ui ca ng truyn t bnh ngng chm xung di b mt ca dung dch hp th. Trong khi nt y ca bnh phn gii vo v tr thch hp, trn k lng cc cht bng cch cun xay. Ngay lp tc bt u chng ct v tip tc tc n nh cho n khi thu c 200 cm3 phn ct. Nu mu ca cht ch th thay i, ch th kim ca dung dch hp th, nh ch vic xc nh v lp li cc thao tc v dng nhiu axit sunfuric hoc phn mu th nh hn. Khi chng ct han thnh (thng th tch trong bnh tj khang 300 cm3), chun cc cht bng dung dch natri hydroxit, c trn buret chnh xc n 0,02 cm3. +Hp th bng axit boric: Cho 100 cm3 dung dch axit boric vo bnh cha ca thit b chng ct vi hai git dung dch hn hp cht ch th. Tin hnh chng ct nh m t phn hp th bng axit sunfuric v chun phn ct bng dung dch axit sunfuric, c trn buret chnh xc n 0,02 cm3. _ song song vi vic xc nh, tin hnh php th mu trng vi cng lng thuc th trong cng iu kin th nghim, nhng b qua phn mu th. 2.1.3.7. Cng thc tnh Khi axit sunfuric c s dng lm dung dch hp th, hm lng nit ca cao su c tnh bng phn trm khi lng theo cng thc: 0,14 x (V2 V1)/m Trong : V1 th tch dung dch natri hidroxit dng chun (cm3) V2 th tch dung dch natri hidroxit dng chun trong php th mu trng (cm3) m khi lng ca phn mu th (g) Kt qu c tnh chnh xc n 0,01 % Khi axit boric c s dng l dung dch hp th, hm lng nit ca cao su c tnh bng phn trm khi lng theo cng thc:

0,14 x (V3 V4)/m Trong : V3 th tch dung dch axit sunfuric dng chun (cm3) V4 th tch dung dch axit sunfuric dng chun trong php th mu trng (cm3) m khi lng ca phn mu th (g) Kt qu c tnh chnh xc n 0,01 % 2.2. Phn tch cc ch tiu ha hc trong cao su latex 2.2.1. Phn tch hm lng cht rn 2.2.1.1. Phm vi p dng Tiu chun ny qui nh phng php xc nh tng hm lng cht rn ca latex cao su thin nhin c c, cc loi cao su tng hp. Phng php ny khng thch hp cho cc loi latex c ngun gc thin nhin khc vi Hevea brasiliensis hoc latex phi liu, latex lu ho hoc cao su khuych tn nhn to. 2.2.1.2. Nguyn tc Mu th c sy n khi lng khng i trong mt t sy di cc iu kin c qui nh p xut kh quyn, tng hm lng cht rn c xc nh bng cch cn trc v sau khi sy. 2.2.1.3. Thit b _ Cc dng c thng thng dng trong phng th nghim _ a y phng, thnh thp, ng knh khong 60 mm, c np y. _ T sy, c th duy tr nhit 700C 20 C hoc 1050C 50C 2.2.1.4. Cch tin hnh _ Cn a c np y chnh xc n 1 mg. Rt vo a 2,0 g 0,5 g latex, y np li v cn chnh xc n 1 mg , lng nh a latex ph y a. Nu cn thit rt vo a khong 1 nc ct hoc nc c tinh khit tng ng v trn u vi latex bng cch lc nh.

_ t a m np nm ngang vo trong t sy ( 4.2) v sy 700C 20C _ Sy p sut thp c xem nh phng php khng thch hp 2.2.1.5. Cng thc tnh Tng hm lng cht rn ( TSC) c tnh bng phn trm khi lng theo cng thc: m1/m0 x 100 Trong : m0 l khi lng ca mu th (g) m1 l khi lng mu th sau khi sy (g) Sai lch kt qu ca hai ln th lp li khng ln hn 0,2 % ( m /m) 2.2.2. Phn tch hm lng cao su kh 2.2.2.1. Phm vi p dng _ Xc nh hm lng cao su ca latex cao su thin nhin c c. _ Phng php ny khng thch hp cho cc loi latex c ngun gc thin nhin khc vi Heavea brasiliensis hoc latex phi liu, latex lu ho hoc cao su khuych tn nhn to v cng khng p dng i vi cao su tng hp. 2.2.2.2. Nguyn tc Mu th c pha long n 20 % tng hm lng cht rn v ng kt bng axit axetic. Cao su ong c cn thnh t v sy kh 700C. 2.2.2.3.Thuc th Trong qu trnh phn tch, ch s dng cc loi thuc th loi tinh khit phn tch v nc ct hoc loi nc c tinh khit tng ng Dung dch axit axetic, 20 g /dm3 (dng cho latex c c c bo qun bng amoniac) Dung dch axit axetic, 50 g/dm3 ( dng cho latex c c c bo qun bng amoniac) Thm 50 g axit axetic m c vo 500 cm3 ca propan 2- ol v pha long vi nc dn 1 dm3 2.2.2.4. Thit b

_ Dng c thng thng dng trong phng th nghim _ a, tt nht a thu tinh hoc s c ng knh khong 100 mm v su 50 mm _ a nhm khng thch hp cho loi latex c c c cha kali hydroxyt 2.2.2.5. Cch tin hnh _ Nu cha bit tng hm lng cht rn th xc nh n _ Th nghim c lp li hai ln _ Cn 10 g 1 g mu th trong l cn, chnh xc n 1mg. Rt vo a thm nc vo y a gim tng hm lng cht rn ca mu th xung n 20 % 1% ( m/m). Xoay u a trn mt phng lm ng u mu th. Tip tc theo mt trong hai trng hp sau _ Trong trng hp latex c c c bo qun vi amoniac, thm vo 75 cm3 5 cm3dung dch axit axetic 20 g/ dm3 ( 5.1) trong thi gian 5 pht bng cch rt t t axit vo di y a v xoay nh n nh t cao su ng di b mt axit.y bng mt knh ng h v gia nhit trn bp cch thu khong 15 pht n 30 pht. Nu serum cn c, thm 5 cm3 etanol 95 % ( V/V). _ Trng hp latex c c c bo qun vi kali hydroxyt thm 25 cm3 5 cm3 dung dch axit axetic 50 g /dm3. Trn u mu th bng a thu tinh v ra sch bng nc ct tt c latex dnh vo a c cho vo a. _ n nh t cao su ng di b mt axit.y a bng mt knh ng h v gia nhit trn bp cch thu khong 15 pht n 30 pht. _ Khi serum trong li, gp cc mnh ng nh vo ming ng chnh. Ra cao su ng trong nc nhiu ln cho n khi nc khng cn axit khi th bng giy qu. _ p cao su ng nc thot ra v to thnh t ng u dy khng qu 2 mm. Mt cch thch hp khc cao su ng trn mt a thu tinh v dng nt thu tinh c ng knh 45 mm hoc vt tng t p ming cao su ng t ngoi vo trong.

_ Ra k t cao su di vi nc t nht 5 pht nu latex c c c bo qun vi amoniac hoc t nht l hai gi nu bo qun vi kali hydroxyt. t cao su ro nc t nht 5 pht trc khi a vo t sy. _ Sy t cao su nhit 700 C 20 C cho ti khi ht mu trng. Nu t cao su c sy trn ming knh ln, cn thn tr t cao su hai n ba ln trong vi gi sy u tin. Lm ngui trong bnh ht m ri cn. Lp li thao tc sy, lm ngui, cn cho n khi khi lng mt i t hn 1 mg sau khi sy 30 pht. _ Nu t cao su b dnh v b nghi oxit ho tc ng xy ra 700C, th gim nhit sy thp hn . V d nh 550C. 2.2.2.6. Cng thc tnh Hm lng cao su kh ( DRC ) ca latex c c c tnh bng phn trm trn khi lng theo cng thc sau: DRC =m1/ m0 x 100 Trong : m0 l khi lng ca mu th (g) m1 l khi lng ca t cau su kh (g) Mi kt qu ca hai ln th so vi gi tr trung bnh khng c ln hn 0,1 % ( m / m). Nu khng ng cn lp li php th. 2.2.3.Xc nh hm lng cn 2.2.3.1. Phm vi p dng _ Xc nh hm lng cn ca latex cao su thin nhin c c. _ Phng php ny ch ph hp vi latex t ngun gc Hevea brasiliensis, khng thch hp cho latex phi liu hoc latex lu ha. 2.2.3.2. Nguyn tc Mt mu th c ly tm v phn cn c c ra nhanh vi dung dch cn ammoniac. Cn c sy kh n khi lng khng i. 2.2.3.3. Thuc th

_ Trong sut qu trnh, ch c s dng cc loi ha cht tinh khit phn tch v ch dung nc ct hay nc c tinh khit tng ng. _ Dung dch ammoniac v cn, c cc thnh phn nh sau: _ Dung dch ammoniac, p= 0.90g/cm3 0.02g/cm3 10 cm3 340 cm3 1000 cm3

_ Etanol tinh khit ti thiu 95% (V/V) _ Nc 2.2.3.4. Dng c v thit b _ Cc dng c thong thng dng trong phng th nghim

_ My ly tm c gia tc trung bnh khong 12000 m/s2 c hai ng ly tm hnh nn 50 cm3. _ Pipet, dung dch thch hp, ng knh ming ht vo khong 2mm 2.2.3.5. Cch tin hnh Tin hnh vic th nghim bng giy i, dung hai ng ly tm (5.1) i trng nhau. Cn latex c c t 40g n 45g, chnh xc n 0.1g v cho vo mi ng. X l mi ng nh sau: y ming ng ngn nga s to mng trong khi ly tm v ly tm khong 20 pht vi gia tc trung bnh 12000 m/s2. Vt ht lp kem v dung pipet (5.2) ly ra phn cht lng ni cch b mt cn khong 10mm. Cho dung dch cn ammoniac gn cht lng pha trn, nh du vch 10mm v chuyn cn ti mt chn chu nhit c dung tch khong 200cm3. Lm bay hi cho n cn v sy kh 700C 20C cho n khi khi lng b mt nh hn 1 mg trong vng 30 pht. 2.2.3.6. Cng thc tnh Hm lng cn tnh bng phn trm khi lng theo cng thc: m1/m0 x 100 Trong : m0 l khi lng ca mu th, tnh bng gam m1 l khi lng ca cht cn sy kh, tnh bng gam Sai lch gia hai kt qu khng c vt qu 0.002% 2.2.4. Phn tch hm lng kim

2.2.4.1. Phm vi p dng _ Xc nh kim ca latex cao su thin nhin c c. _ Phng php ny khng thch hp cho cc loi latex c ngun gc thin nhin khc vi Hevea brasiliensis hoc cc loi latex cao su tng hp, latex phi liu, latex lu ha hoc cao su phn tn nhn to. 2.2.4.2. Nguyn tc _ Phn mu th latex c c c chun bng axit n pH 6 vi s c mt ca cht n nh trnh s ng t bng phng php chun in th hoc cht ch th mu metyl . kim c tnh t lng axit s dng. 2.2.4.3. Thuc th _ Dung dch n nh: dung dch 5% (theo khi lng) ca cht n nh khng ion loi ngng t alkyl phenol polyetylen oxit. Trc khi s dng, pH ca dung dch phi c iu chnh n tr s 6.0 _ Axit sulfuric, c = 0.05 mol/dm3, hoc axit clohydric, c = 0.1 mol/dm3 _ Metyl , dung dch 0.1% trong etanol c tinh khit khng nh hn 95% (theo th tch). 2.2.4.4. Thit b, dng c _ My khuy in c cnh khuy phi kim loi, hoc my khuy t _ Thit b o pH _ Cn 2.2.4.5.Cch tin hnh _ Ly khong 200mL nc vo trong mt cc thy tinh dung tch 400mL, trong khi khuy thm vo 10mL dung dch n nh. Cho 5 10g latex c c vo trong l cn v khut u. Bo m latex c cho vo khng b chy xung thnh cc thy tinh (c th dn n tht thot amoniac) hoc xung thnh l cn _ Lp in cc ca thit b o pH v khuy lin tc, dng buret thm dung dch axit sulfuric hoc axit clohydric cho n khi pH gim ti tr s 6.0. Khi gn n im cui thm tng git axit. _ Nu khng dng phng php chun in th th dng metyl lm cht ch th, ghi li im cui khi mu i sang hng.

2.2.4.6. Cng thc tnh Ty thuc vo latex c c c bo qun bng amoniac hay kali hydroxit, tnh ton b kim tng ng theo quy nh sau y. _ Nu latex c c c bo qun bng amoniac, kim c tnh bng % (theo khi lng) amoniac (NH3) trong latex c c, theo cng thc kim (theo NH3) = F1CV / m Trong F1 l h s 1.7 i vi axit clohydric hoc 3.4 i vi axit sulfuric C l nng thc ca axit clohydric hoc sulfuric s dng, tnh bng mol/dm3 V l th tch axit s dng, tnh bng cm3 m l khi lng ca phn mu th, tnh bng gam Bo co kt qu l gi tr trung bnh ca hai ln th. Nu cc kt qu ring l sai lch ln hn 0.01 n v so vi gi tr trung bnh khi kim thc t ln hn 0.5 n v, hoc sai lch ln hn 0.005 n v so vi gi tr trung bnh khi kim thc t khng ln hn 0.5 n v, lp li php xc nh. _ Nu latex c c c bo qun bng kali hydroxit, kim c tnh bng % kali hydroxit (theo khi lng) trong latex c c, theo cng thc: kim (theo KOH) = F1CV / m Trong F1 l h s 5.61 i vi axit clohydric hoc 11.22 i vi axit sulfuric C l nng thc ca axit clohydric hoc sulfuric s dng, tnh bng mol/dm3 V l th tch axit s dng, tnh bng cm3 m l khi lng ca phn mu th, tnh bng gam

Bo co kt qu l gi tr trung bnh ca hai ln th. Nu cc kt qu ring l sai lnh ln hn 0.015 n v so vi gi tr trung bnh, lp li php xc nh. 2.2.5. Phng php xc nh tr s axit bo bay hi 2.2.5.1. Phm vi p dng Tiu chun ny qui nh phng php xc nh tr s axit bo bay hi ca latex cao su thin nhin c c. Phng php ny khng thch hp cho cc loi latex c ngun gc khc vi Hevea brasiliensis hoc latex phi liu, latex lu ha, khuch tn nhn to hoc cc loi latex tng hp. 2.2.5.2. nh ngha Tr s axit bo bay hi (VFA) ca latex c c: s gam kali hydroxyt tng ng trung ha lng axit bo bay hi trong mu latex c c cha 100g tng cht kh. 2.2.5.3. Nguyn tc Mt mu th c lm ng c bng amoni sunfat v mt phn mu serum to thnh c tch ra v c axit ha vi axit sunfuric. Serum axit ha c chng ct bng hi v xc nh cc axit bo bay hi c mt trong mu th bng cch chun cht ngng t vi dung dch bari hydroxyt chun. 2.2.5.4. Thuc th Trong qu trnh phn tch, ch s dng nhng thuc th c cht lng tinh khit v nc ct hoc nc c tinh khit tng ng. _ Dung dch amoniac sunfat khong 30% _ Dung dch axit sunfuric khong 50% _ Dung dch bari hydroxyt tiu chun, 0.005 mol/dm3 c chun ha bng cch nh phn vi kali hydro phtalat v c bo qun trong iu kin khng c cacbon dioxit. _ Dung dch ch th: cng vi dung dch bromothylmol xanh hoc phenolphtalein 0.5% trong hn hp ng th tch tng ng ca etanol v nc. 2.2.5.5. Thit b

Cc dng c thng thng dng trong phng th nghim. _ Dng c chng ct _ B chng cch thy _ Pipet c dung tch 5cm3, 10cm3, 25 cm3 v 50 cm3 _ Buret c dung tch thch hp 2.2.5.6. Cch tin hnh _ Cn 50g latex c c trong ly thy tinh, dng pipet thm chnh xc 50cm 3 dung dch amoni sunfat v dng a thy tinh va khuy va cho thm. t ly thy tinh cha mu trn b chng cch thy nhit 70oC v tip tc khuy cho n khi latex ng li. Dng mt knh ng h y ly li v yn n trong hoc trn b chng cch thy trong khong thi gian 15 pht. Tch serum bng cch p xon latex ng qua giy lc kh. Dng a thy tinh p cc latex ng ly tip phn serum cn li. Sau lc serum qua cng loi giy lc. Ht 25cm3 serum lc cho vo trong bnh nn kh dung tch 50cm3 v axit ha n bng cch thm vo 5cm3 dung dch axit sunfuric v lc u. _ c bit mt vi loi latex c c c bo qun bng kali hydroxyt, mt s kt ta nh c th to nn trong giai on axit ha. Cht kt ta ny phi c ly ra bng cch lc qua giy lc kh mi trc khi tin hnh chng ct. _ Cho hi nc i qua dng c chng ct t nht l 15 pht. Hi nc i qua v bn ngoi ca dng c. Dng pipet cho 10cm3 serum axit ha vo ng trong, nu c bt gy tr ngi th c th thm mt git cht chng bt thch hp. t ng ong 100cm3 c khc vch di u b phn ngng t thu cht ngng t. ng t t lung hi nc i hng hi i vo ng chng ct. u tin cho hi t t vo, sau ng ton b hi i ra v tip tc chng ct tc 3cm3/pht cho n khi thu c 100cm3 cht ngng t. _ Chuyn cht ngng t c vo mt bnh hnh nn dung tch 250cm3 v loi b tt c cacbon dioxit ha tan khi cht ngng t bng cch cho mt dng kh khng c cacbon dioxit tc 200cm3/pht n 300cm3/pht khong 3 pht. Chun bng dung dch bari hydroxyt, dng vi mt trong cc cht ch th mu. _ Tin hnh lp li th nghim vi 50g mu latex c c mi.

2.2.5.7. Cng thc tnh

134.64cV m(100 DRC 50 + mTSC 100

VFA =

Trong : C l nng thc t ca dung dch bari hydroxyt, tnh bng mol/dm3 V l th tch ca dung dch bari hydroxyt cn thit trung ha cht ngng t, tnh bng cm3. DRC l hm lng cao su kh ca latex c c, tnh bng phn trm khi lng m l khi lng ca mu th, tnh bng gam p l t khi ca serum, tnh bng megagam/m3, p 1.02 mg/m3 i vi latex c c ly tm hoc kem ha TSC l tng hm lng cht rn ca latex c c tnh bng phn trm khi lng 134.64 l h s dn xut pht t khi lng phn t tng i ca kali hydroxyt, n tng ng vi bari hydroxyt v cc phn khc ca serum c axit ha v chng ct. Lp li th nghim nu kt qu ca hai ln th khng tha mn vi: _ Trong phm vi 0.01 n v nu tr s VFA thc t khng ln hn 0.10 n v _ Trong phm vi 10% nu tr s VFA thc t ln hn 0.10 n v 2.2.6. Phng php xc nh tr s KOH 2.2.6.1. Phm vi p dng Xc nh tr s KOH ca latex cao su thin nhin c c c bo qun ton b hay mt phn bng amoniac. Phng php ny c th p dng cho cc loi latex c cha axit boric. Phng php ny khng p dng cho cc loi latex bo qun bng kali hydroxit. Phng php ny khng thch hp vi cc loi latex c

ngun gc t nhin khc vi Hevea brasiliersis hoc cao su tng hp, latex phi liu, latex lu ha hoc cao su phn tn nhn to. 2.2.6.2. nh ngha Tr s KOH l s gam kali hydroxit tng ng vi lng axit c lin kt vi amoniac trong latex cha 100g tng hm lng cht rn. 2.2.6.3. Thuc th Trong qu trnh phn tch, ch dng cc loi ha cht c cht lng tinh khit phn tch v ch dng nc ct khng cha cacbon dioxit ha tan hay nc c tinh khit tng ng _ Kali hydroxit, 0.1 mol/dm3, khng cha cacbonat _ Kali hydroxit, 0.5 mol/dm3, khng cha cacbonat _ Formaldehyt, 45 g n 50 g trong 1 lt dung dch, c = 1.5 mol/dm3 n 1.67 mol/dm3, khng cha axit, c chun b bng cch pha long formaldehyt m c vi nc v trung ha bng dung dch kali hydroxit, s dng khi cht ch th phenolphtalein chuyn sang mu hng nht. _ Cch xc nh hm lng formaldehyt a. Thuc th _ Natri sulfit, khan, loi tinh khit phn tch _ Axit sulfuric 0.25 mol/dm3 _ Thymolphtalein, dung dch ch th. Ha tan 80 g thymolphtalein trong 100mL ru etyl v pha long vi 100mL nc ct. b. Cch tin hnh Chun b mt dung dch 125 g natri sulfit khan trong 500mL nc v pha long n th tch 1lt. Chuyn 100mL dung dch vo bnh nn dung tch 500 mL. Cn chnh xc t 6.0g n 8.0 g dung dch formaldehyt c nng 50 g/dm3 cho vo bnh nn v lc trn k. yn trong 5 pht, sau chun vi axit sulfuric 0.25 mol/dm3 n im cui khi dung dch chm mt mu dng thymolptalein lm cht ch th. Tin hnh xc nh mu trng vi dung dch natri sulfit. c. Cng thc tnh

Tnh hm lng formaldehyt ca dung dch formaldehyt bng phn trm khi lng theo cng thc:

30.03(V1 V2 ) 2C H 2 SO4 10m1

Trong : V1 l th tch ca axit sulfuric dng chun mu th ca dung dch formaldehyt, tnh bng mL. V2 l th tch ca axit sulfuric cn thit dng trong mu trng, tnh bng mL. CH2SO4 l nng thc ca axit sulfuric, tnh bng mol/dm3 m1 l khi lng mu th ca dung dch formaldehyt 2.2.6.4. Cch tin hnh Cn phn mu th c cha khong 50g tng cht rn vo cc thy tinh 400mL, cn chnh xc n 0.1g. Nu cn thit, iu chnh kim ti (0.5 0.1)% amoniac c tnh theo phn nc bng cch thm v khuy mt lng cn thit dung dch formaldehyt Tnh th tch dung dch formaldehyt c thm vo bng mL theo cng thc sau

m(100 WTS )( A 0.5) 113 .4 CHCHO

Trong CHCHO l nng thc ca dung dch formaldehyt, tnh bng mol/dm3 WTS l tng hm lng cht rn A l kim _ Pha long latex bng nc n khong 30% tng cht rn _ Nhng in cc ca thit b o pH vo latex c c pha long v ghi pH

_ Nu pH ban u nh hn 10.3, thm t t 5mL dung dch kali hydroxyt 0.5mol/dm3 trong khi khuy chm bng my khuy t. Ghi pH c c trng thi cn bng. Tip tc khuy v thm mi ln (15 giy) 1mL dung dch kali hydroxyt nng 0.5 mol/dm3, ghi li pH trng thi cn bng sau mi ln cho thm. Tip tc cho n khi t c im cui. _ Nu pH ban u l 10.3 hoc ln hn, khng thm mt ln 5mL nh lc ban u, trc tip thm mi ln 1mL dung dch kali hydroxyt 0.5mol/dm3. _ im cui ca php chun l im un ca ng cong chun c gi tr pH da vo th tch dung dch kali hydroxyt, tnh bng mL. Ti thi im ny, dc ca ng cong, tc l chnh lch u tin, t cc i v chnh lch th hai thay i t gi tr dng sang gi tr m. im cui s c tnh t chnh lch th hai do tha nhn rng s thay i t gi tr dng sang gi tr m chu s tng quan tuyn tnh trong khong 1mL ca kali hydroxyt thm vo. Chnh lch gia 2 ln th nghim khng qu 5% (theo khi lng) V d v php chun in hnh ch ra s thay i pH Th tch dung dch KOH c thm vo mL Ban u 5 6 7 8 9 10 11 12 Tr s pH 10.09 10.46 0.09 10.55 0.10 10.65 0.11 10.76 0.14 10.90 0.18 11.08 0.24 11.32 0.31 11.63 0.30 -0.01 0.07 0.06 0.04 0.03 0.01 0.01 chnh lch u tin pH/mL chnh lch th hai 2pH/mL

13 14

11.93 0.21 12.14

-0.09

Trong v d ny, chnh lch th nht t cc i l 0.31 gia 11mL v 12mL dung dch kali hydroxyt. im un chnh xc ca ng cong chun c tnh t t l ca gi tr chnh lch th hai lin k, c ngha l 0.07/ (0.07+0.01) = 0.875 chnh lch gia 11mL v 12mL, c ngha l 11.875mL

2.2.6.5. Cng thc tnh Tr s KOH ca latex cao su thin nhin c c c tnh bng % khi lng theo cng thc sau:

51 C 6 V WT m S
Trong : C l nng thc ca dung dch kali hydroxyt, c biu th bng s phn t gam KOH/dm3

V l th tch ca dung dch kali hydroxyt 0.5mol/dm3 cn thit t ti im cui, tnh bng mL WTS l tng hm lng cht rn ca latex c c, tnh bng % khi lng m l khi lng ca phn mu th, tnh bng gam. _ Nu latex c c cha axit boric, th ly tr s KOH xc nh tr i tr s KOH tng ng ca axit boric hin c. Tnh tr s KOH tng ng vi axit boric hin c theo cng thc

W 9 BA 1 WTS
Trong WBA l hm lng axit boric, c tnh bng % khi lng. 2.2.7. Phn tch hm lng ng 2.2.7.1. Phm vi p dng p dng phng php quang ph xc nh tng lng vt ca ng trong cao su th, latex v cao su phi liu, cho c cao su thin nhin v cao su tng hp. Phng php ny c th p dng cho cao su cha silic, vi iu kin l c x l bng axit flohydric trong qu trnh th. Phng php ny c nhy nh hn 1mg ng / kg. 2.2.7.2. Nguyn tc Mu cao su c tro ho hay phn hu trong hn hp axit nitric v axit sunfuric m c. Sau loi s lng canxi tha ( nu c ) v to phc vi bt k cht st no vi s c mt ca amoni xitrat. Sau kim ho, dung dch tch ra c trn vi mt dung dch dietyldithiocarbamat 1.1.1 tricloroetan to thnh v tch ra phn phc hp mu vng ca ng. Dung dch ny c o bng phng php quang ph k v so snh vi kt qu o dung dch chun thch hp trn, t xc nh hm lng ca ng. 2.2.7.3. Thuc th v vt liu

Trong sut qua trnh phn tch, ch s dng loi ho cht tinh khit phn tch v ch dng nc ct hay nc c tinh khit rng ng. _ Natri sunfat khan _ Axit sunfuric m c , = 1,84 g / cm3. _ Axit nitric m c, = 1,42 g / cm3. _Hn hp axit clohydric v axit nitric, c iu ch nh sau: Trn vi nhau : + 2 th tch axit clohydric, = 1,18 g /cm3 + 1 th tch axit nitric, = 1,42 g /cm3 + 3 th tch nc. _ Hydro peroxit , 30 % _ Dung dch amoniac , = 0,890 g / cm3 _ Axitclohydric, c( HCl) = nng 5 mol / dm3 _ Axit fluohydric, = 1,13 g/cm _ Dung dch axit xitric Ho tan 50 g axit xitric trong 100 cm3nc. _ Dung dch km dietyldithiocarbamat + Ho tan 1g km dietyldithiocarbamat rn trong 1000 cm31.1.1 tricloroetan. Nu km dietyldithiocarbamat trong nc v thm 2 g km sunfat heptahydrat. Phn chit ra c km dietyldithocarbamat c trn vi 1000 cm3 vi 1.1.1 tricloroetan. Dung dch ny bn t hn 6 thng khi c bo qun trong chai thu tinh khng b phn quang _ ng, dung dch chun cha 0,01 g Cu / dm3 + Cn 0,393 g ng sunfat pentahydrat ( CuSO4.5 H2O) cho vo mt ly nh v ho tan trong nc. Thm vo 3 cm3 axit sunfuric m c( 4.2), chuyn dung dch qua bnh nh mc 1000 cm3 (5.6) v pha long vi nc ti vch lm dung dch d tr. Dng pipet ht 10 cm3 dung dch d tr vo trong bnh nh mc 100 cm3 ( 5.6) v pha long vi nc ti vch nh mc. 1 cm3 ca dung dch ny cha 0,01 mg Cu. iu ch mi t ngun dung dch d tr khi cn thit _ Magie oxit

_ Giy qu _ Giy lc ( loi giy cng, khng axit) 2.2.7.4. Thit b _ Dng c thng thng dng trong phng th nghim _ My quang ph hp th hoc quang ph k c kh nng o mt quang di sng khong 435 nm ng vi ng so mu thch hp c di l 10 mm. _ Bnh Kendan c dung tch 100 cm3 bng silic hay thu tinh boro silicat _ Chn s hay a s, silic hay platin, dung tch 50 cm3 i vi mu nh hoc dung tch ln hn i vi mu ln hn. c bit l bng s hay silic nu b n mn nn bi khong 0,1 g magie oxit, bi phn y v mt phn thnh xung quanh. Vic lm ny hn ch thp nht kh nng ng hp nht kh nng ng hp th qua vch b n mn v cc cht n ( nu c ) thay vo magie oxit s b hp th. Nu dng dng c bng platin th khng cn x l bng magie oxit. _ Pipet, 25 cm3 _ Cn phn tch, chnh xc n 0,1 mg _ Bnh nh mc, mt vc dung tch 100 cm3 v1000 cm3 _ Bp in hoc bp ct _ a khuy, bng platin 2.2.7.5. Cch tin hnh Tin hnh lp li th nghim hai ln. _ Mu th rn cn phi chun b bng cch cn mu (1 ) v / hoc chia nh ( 2) (1) Cn mu 6 ln gia hai ng cn ngui ca my cn phng th nghim c khe h gia hai trc l 0,5 mm, cun trn mu cao su mi ln cn v tr u cun cao su cho ln cn tip theo. (2) Ct mu thnh tng mng nh khng ln hn 0,1 g. _ Cn chnh xc n 1 mg mt mu th c khi lng t 2 g n 10g , trong trng hp mu rn phi chun b theo (1)

_ C mu th ph thuc vo lng ng c mt trong mu c th c chn sao cho c mc hp th c t 0,3 n 0,8 n v; trong trng hp hm lng ng rt thp, s c gim 10 ln ca thang hp th , c mu th thch hp s tu thuc vo kinh nghim. _ Ho tan mu th o ng phi c tin hnh bng cch tro ho (3) hay cng ph mu th bng axit (4). Nu cao su cha clorin nn dng phng php cng ph mu bng axit (4). (3)Tro ho phn mu th theo ng phng php A hay phng php B. Sau tro ho lm t tro bng 0,5 cm3 ti 1 cm3 nc, sau thm 10 cm3 hn hp axit y bng mt knh ng h v t vo khong 1000 C t 30 n 60 pht. Nu tro tan hon ton , chuyn lng dung dch vo mt bnh tam gic nh. Nu tro ho khng hon ton hoc nu c mt silicat bit tip tc lm nh sau: _ Dng mt mu th mi v mt chn platin mi. Lp li s tro ho theo ng phng php A hay phng php B. Sau khi tro ho, thm vo vi git axit sunfuric v un cho bc hi. ngui v thm vo ba git axit sunfuric na v 5 cm3 axit fluohydrric. un trn bp in hay bp ct khuy bng a platin v lm bay hi n kh cn. Lp li qu trnh ny hai ln hoc lm cho n khi nhn thy ton b silicat bin mt, khi y khng cn khi trng ca silicon tetrafluorid. ngui, lm t chn tro vi mt lng t 0,5 cm3 ti 1 cm3 nc, thm 10 cm3 hn hp axit cm3 y kn bng mt ng h v un 1000C t 30 n 60 pht, chuyn lng dung dch vo trong bnh tam gic nh. (4) Cng ph mu th vi 4 cm3axit sunfuric v 3 cm3axit nitric trong bnh Kendan . Lm m bnh bt u s phn ng. Lng ho cht cho mt mu th l 2 g. Nu dng mu th ln hn th cn lng axit nhiu hn. _ Nu phn ng tr nn qu mnh, lm ngui bnh trong mt ly nc lnh. Khi phn ng ban u gim, un nh hn hp cho n khi ngng phn ng mnh v k n un mnh hn na cho n khi hn hp sm mu. Thm 1 cm 3axit nitric, un nng hn hp sau mi ln thm axit cho n khi hn hp sm mu.

Tip tc thao tc ny cho n khi dung dch tr nn khng mu hoc c mu vng nht v khng lm sm mu khi un thm na. Nu vic phn hu mu b ko di, cn phi thm khong 1 cm3 axit sunfuric n ngn chn hn hp b ng rn. Ph hu hon ton cc vt hu c, ngui hn hp v thm 0,5 cm3 hydro peroxit v hai git axit nitric. Sau un dung dch cho bc hi, lp li vic thm vo v un cho n khi mu ca dung dch khng cn gim na. Lm ngui dung dch, pha long vi 10 cm3 nc v lm bay hi. Cui cng lm ngui dung dch v thm vo 5 cm3 nc. _ Nu dung dch th giai on ny khng c cht khng ho tan, chuyn axit cng ph mu ti mt bnh tam gic. Tuy nhin nu dung dch th cha cht khng ho tan, lc phn dung dch bn trn qua mt t giy lc nh vo trong bnh tam gic, gi li cng nhiu cng tt cht khng tan cn li trong bnh Ken dan, un dung dch n si v lc mnh thnh bnh. Lc qua giy lc vo bnh tam gic.Ra bnh Kendan i ba ln mi ln 5 cm3nc, chng cng c gom vo bnh. _ Sau khi thc hin cc giai on (3) hoc (4) thm 5 cm3 dung dch axit citric vo trong bnh tam gic v nu khi lm ngui, dung dch vn trong, trung ho n bng cch thm vo tng git dung dch amoniac dng mt ming giy qu nh lm cht ch th. Nu canxi sunfat kt tinh bn trong dung dch khi lm ngui, th lm lnh bnh v hn hp ti khong 100C, lc vo trong bnh tam gic th hai, ra v lc ba ln, mi ln 2 cm3 nc lnh trc khi trung ho bng dung dch amoniac . Lm ngui dung dch, v d bng cch ngm vo dng nc chy lin tc, chuyn vo mt phu tch, thm vo 2 dung dch amoniac na v sau thm nc pha long khong 40 cm3. Dng ng ht thm 25 cm3 km dietyldithiocarbamat cho vo dung dch v lc 2 pht. Ngay sau khi tch lp, chit lp 1.1.1 tricloroetan vo trong bnh c nt y cha 0,1 g natri sunfat khan. Nu dung dch cn c sau khi yn 30 pht th thm cht t natri sunfat khan cho n khi dung dch tr nn trong.. _ Lc dung dch 1.1.1 tricloroetan qua lp bng thu tinh hay giy lc nh v cho vo ng mu ca my quang ph hp th hoc quang ph k v o mt

hp th ti vng c bc sng dng trong vic chun b v th dng cho 1.1.1 tricloroetan vo ng so mu i chng. Hiu chnh s c bng cch tr i hp th ca dung dch mu trng. _ Tin hnh xc nh mu trng bng cch dng v ng cch lng ho cht thch hp, nhng khng c phn mu th .Mu trng khng c ln hn 2 mg Cu / kg. 2.2.7.6. Dng ng cong chun _ Chun b mt lot dung dch chun, mi dung dch cha 5 cm 3 axit sunfuric c pha long vi 10 cm3 nc . Thm vo mi dung dch ny mt lng dung dch ng chun thay i t 0 n 10 cm3, sau thm 5 cm3 dung dch axit xitric. Thm tng git dung dch amoniac cho n khi dung dch va c tnh kim vi giy qu _ Lm ngui dung dch v chuyn vo mt phu tch ring bit v thm vo mi dung dch 2 cm3 dung dch amoniac na. Dng mt pipet thm vo mi dung dch 25 cm3 ho cht km dietyldithiocarbamat v lc trong 2 pht. Ngay sau khi tch lp, chit lp 1.1.1 tricloroetan vo mt bnh c np y cha khong 0,1 g natri sunfat khan. _ Nu magie oxit c s dng tro ho mu th s lng tng t nn c th trong mi dung dch chun thm vo mt lng tng ng. _ Tng dung dch 1.1.1 tricloroetan ny c lc qua lp bng thu tinh hay giy lc nh vo trong ng so mu ca my quang ph hp th hay quang ph k v o hp th ti bc sng hp th cc i ( bc sng khong 435 nm ), dng 1.1.1 tricloroetan vo ng mu i chng. Hiu chnh s c bng cch tr i hp th ca dung dch khng cha ng. _ nh du trn th c c tng nng tng ng thch hp ca ng v th, m th phi c kim tra mt cch u n theo cc iu kin c th v loi ca thit b c s dng. 2.2.7.7. Biu th kt qu _ Bng th hiu chun, xc nh nng ca ng tng ng vi tr s hiu chnh v t tnh ton ra hm lng ng ca mu th nghim.

_ Kt qu c tnh bng miligam ng/ kg. _ Kt qu l gi tr tring bnh ca kt qu hai ln th nghim 2.2.8. Phn tch hm lng Mangan 2.2.8.1. Phm vi p dng Cc phng php quang ph xc nh mangan sau qu trnh oxy ha vi natri periodat trong cc loi cao su latex. Cc phng php u phn tch cao su c cha clorua. iu 3 quy nh phng php p dng cho cao su phi liu hoc cao su lu ha, phng php khng b nh hng bi cc cht n tr c khi lng nng chng hn nh silicat t nhin v tng hp hoc cc dng canxi cacbonat khc nhau, hoc bi s c mt ca cc cht phi liu to thnh phosphat khng ha tan trong cc iu kin th nghim. iu 4 quy nh phng php p dng cho cao su th, cao su phi liu v cao su tng hp v cc latex cao su khng cha cc cht n nng (ln hn khong 10%) ca cht n tr silicat hay bt k cht no chng hn nh titan dioxit trong cc iu kin th nghim s to thnh phosphat khng tan. 2.2.8.2. Nguyn tc a. Phng php chung Dng cho mu khng b nh hng bi cc cht n nng _ Trng hp mu th c clo: phn hy cao su vi axit sulfuric, sau cho phn ng vi axit nitric. Qu trnh ny c thc hin trong bnh Kjeldahl. Nu mu th c silicat, phn mu th phn hy c x l bng axit sulfuric v fluohydric lm bay hi silicon nh l silicon tetrafluorua. _ Trng hp mu th khng c clo: cao su c tro ha trong mt cc platin v x l vi natri fluoroborat. Sau khi ph mu, mangan b oxy ha thnh permanganat bng cch un si vi dung dch natri periodat. Nng mangan c xc nh bng my o quang ph ti bc sng 525 nm. b. Phng php gii hn Gii hn cho mu c cht n nng < 10%

_ Trng hp mu th c clo: phn hy cao su vi axit sulfuric, sau cho phn ng vi axit nitric. Qu trnh ny c thc hin trong bnh Kjeldahl. Nu mu th c silicat, phn mu th phn hy c x l bng axit sulfuric v fluohydric lm bay hi silicon nh l silicon tetrafluorua. Sau khi ph mu, mangan b oxy ha thnh permanganat bng cch un si vi dung dch natri periodat. Nng mangan c xc nh bng my o quang ph ti bc sng 525 nm. _ Trng hp mu th khng c clo: cao su c tro ha trong chn silica. 2.2.8.3. Thuc th Trong qu trnh phn tch, ch dng cc ha cht tinh khit phn tch, ph hp cho vic dng trong phn tch vt kim loi v ch dng nc n nh _ Natri fluoroborat (s dng ring cho phng php chung): Nu loi phn tch tinh khit khng c sn, thuc th ny s c chun b nh sau: ha tan 110 g natri fluoroborat loi k thut trong 100 ml nc m 35
0

C. Sau khi lc qua mt t giy lc lm ngui dung dch n nhit phng v

thm 100 ml etanol 96% (th tch) trong khi khuy. Lc ly cc tinh th kt ta trn t giy lc trong mt ci phu Buchner v loi nc hon ton trong chn khng yu, sau chuyn qua mt chn s y nng hay a thy tinh v sy khong 50 0C trong chn khng. _ Natri periodat. _ Axit sulfuric: p = 1,84 mg/m3 _ Axit nitric: p = 1,42 mg/m3 _ Nc n nh: c mt lt nc, thm vo khong 0,1 g kali permanganate cng vi mt vi git axit sulfuric. Chng ct nc loi b 50 ml phn chng ct u v cui. Phn cn li cho vo bnh thu tinh c nt y. _ Dung dch kali permanganate: khong 30 g/dm3 _ Mangan, dung dch tiu chun, c 10 mg mangan/dm3, c hai cch pha dung dch ny: + Cn 0,720 g kali permanganate (KMnO4) trong mt ci cc nh v ho tan trong nc c cha 2 ml axit sulfuric. Thm nc c bo ho bng sulfua dioxit

(SO2) cho n khi dung dch mt mu. un si dung dch trong 15 pht, lm ngui, chuyn qua bnh nh mc dung tch 500 ml v pha long bng nc ti vch nh mc. + Cn 0,770 g mangan sulfat (MnSO4.H2O) trong mt ci cc nh v ho tan trong nc c cha 2 ml axit sulfuric (p = 1,84 Mg/m3). Chuyn dung dch vo bnh nh mc dung tch 500 ml v pha long ti vch nh mc. Dung dch ny phi n nh t nht l mt thng. _ Ht 10 ml ca dung dch c pha bng mt trong hai phng php trn cho vo mt bnh nh mc dung tch 500 ml v pha long bng nc li mt ln na ti vch nh mc.1 ml ca cc dung dch tiu chun ny cha 0,01 mg mangan. Chun b dung dch ngay trc khi dng. Hyro peroxit: dung dch 30% (th tch) trong nc. Axit flohydric: p = 1,12 Mg/m3. Kali hydro sulfat (s dng ring cho phng php gii hn). Axit sulfuric, dung dch 1 + 19 (s dng ring cho phng php gii hn): pha long 1 th tch axit sulfuric m c (p = 1,84 Mg/m3) vi 19 th tch nc n nh. Axit orthophosphoric (s dng ring cho phng php gii hn): H3PO4 85% (th tch) ti 90% (th tch). 2.2.8.4. Thit b Cc thit b dung c thng thng trong phng th nghim _ Quang k hay quang ph k: c th o hp th bc sng khong 525 nm v cc ng so mu. _ Chn platin (s dng ring cho phng php chung): dung tch dang ngha 30 ml. _ Chn silica (s dng ring cho phng php gii hn): dung tch khong 50 ml, dng trong trng hp mu th khng c clo. _ Chn platin (s dng ring cho phng php gii hn): dung tch khong 80 ml, dng trong trng hp mu th c clo.

_ Tm chu nhit, cch nhit: chiu ngang khong 100 mm v chiu dy khong 6 mm, c mt l chnh gia gi cho chn sao cho hai phn ba ca chn nm di tm cch nhit. _ L nung: c kh nng duy tr nhit 550 0C 25 0C. _ Lc thy tinh: loi xp P40. _ Bp in hoc bp ga vi b ct. _ Bnh Kjeldahl: dung tch 250 ml. _ a platin: dng khuy. 2.2.8.5. Cch tin hnh a. Phng php chung Ly khong 10 g mu cao su latex, sy n khi khi lng khng i v ct thnh tng mnh nh. Tro ha mu th: + i vi mu th khng c clo: _Chuyn phn mu th vo mt chn platin dung tch 30 ml bit trc khi lng, t chn vo l trong tm chu nhit, cch nhit. _ Bt u chun b mt dung dch trng cng mt lc bng cch dng mt cc tng t nhng khng c phn mu th v tip tc x l phn mu th v mu trng trong cng mt phng php ging nhau. _ Gia nhit chn v mu th bng mt ngn la ga nh cho n khi cn li phn than kh, sau chuyn chn vo l nung c duy tr nhit 550 0C 25 0C v nung cho n khi tt c cacbon b oxy ha. _ Lm ngui chn trong bnh ht m, cn chn xc nh khi lng tro v dng pipet sch thm vo mt lng axit sulfuric tng git xung quanh thnh chn lm m u tro. un nh cho n khi ht khi v nung li khong 550 0C trong vi pht. Lp li thao tc trn mt ln na. Sau ly chn ra v lm ngui n nhit phng, thm vo chn 8 phn khi lng ca natri fluoroborat mc ti a l 8 gam, t mt phn khi lng tro. un nh chn trong mt t ht cho n khi hn hp c tan chy hon ton, ri gi yn cho n khi hn hp b nu

chy tr nn trong sut, hay cho n khi khng cn phn ng xy ra na v bt k cht rn khng tan no cng c phn tn trong cht lng nu chy. + i vi mu th c clo: _ t mu th trong bnh Kjeldahl, thm 10 ml axit sulfuric v lm nng n khi phn mu th phn hy. Cn thn thm 5 ml axit nitric. Nu phn ng xy ra qu mnh, lm ngui bnh trong cc cha nc lnh v nhit phng t nht l 2 gii trc khi lm nng li. _ Ngay sau khi phn ng u tin xy ra xong, lm nng nh hn hp cho n khi phn ng dng li, sau lm nng mnh hn cho n khi hn hp ha en. Thm 1 ml axit nitric v un nng cho n khi en tr li. Lp li vic thm axit nitric v un nng cho n khi dung dch tr nn mt mu hay vng nht v tr li mu en khi un lu hn. _ Nu s phn hy ko di, cn phi thm 1 ml axit sulfuric trnh cc cht ha cng trong bnh. _ Nu cht phn hy khng c cht khng ha tan, ngui, thm 0,5 ml hydro peroxit v 2 git axit nitric v lm nng cho n khi bc khi. Lp li vic thm hydro peroxit cho n khi khng c s gim mu trong dung dch. Lm ngui pha long bng 10 ml nc v lm nng cho ti khi bc khi. _ Chuyn dung dch v bt k cht cn no cn li vo chn platin dung tch 30 ml, cho bay hi n kh v t chy cho n khi cacbon chy ht. _ Nu cn nhng cht khng tan trong vic phn hy giai on ny, lm ngui, thm vi git axit sulfuric v 5 ml axit flohydric. Cho bc hi n kh trn bp ng thi khuy a platin. Lp li thao tc ny hai ln. Nu khng c cht khng ha tan, lm bay hi n kh trn bp. Ha tan mu th: _ Lm ngui chn nhit phng, thm 12 ml nc n nh v 4 ml axit sulfuric. Sau khi un nh ha tan cc cht b ng kt, rt ton b mu trong chn vo mt bnh nn dung tch 100 ml. Lp li bc ny vi 10 ml nc n nh v 2 ml axit sulfuric, sau rt ht vo bnh nn.

_ Cho thm 5 ml axit nitric vo bnh v sau rt dung dch qua li lc bng thy tinh sch, ra li lc mt ln bng 5 ml nc n nh nng. Chuyn cht lng c lc qua mt bnh nn khc, ra vi nc n nh, v thm nc c th tch tng cng l 40 ml, thm 0,3 g natri periodat v un si dung dch. Tip tc un si nh trong 10 pht m bo dung dch ln ng mu. Sau khi lm ngui, bt k cht m c no nh kali periodat b kt ta c th lm trong sut bng cch ly tm hay lc qua li lc. _ Chuyn dung dch vo mt bnh nh mc dung tch 50 ml v pha long ti vch nh mc bng nc n nh 20 0C. Sau khi pha, mu sc phi n nh trong vi gi. Bt k tnh hung phai mu no l do vic loi b khng hon ton tp cht hu c v clorua. Nu iu ny xy ra, lp li vic xc nh nhng dng thm axit sulfuric x l ging nh trong tro ha mu th khng c clo. Chun b cc dung dch i chng tiu chun: Chun b mt lot dung dch i chng tiu chun, mi dung dch cha 25 ml nc n nh, 6 ml axit sulfuric v 5 ml axit nitric. T cc dung dch ny, thm phn dung dch mangan tiu chun thay i t 0 ml (dung dch nn) n 10 ml, cng vi mi trng hp thm 0,3 g natri periodat. un si cc dung dch trong 10 pht m bo ln ng mu. Cui cng, lm ngui v pha long bng nc n nh ti 50 ml trong bnh nh mc. Php o quang ph: _ Ra ng so mu ca quang k hay quang ph k trc tin bng dung dch kali permanganat, sau vi nc n nh v sau cng l dung dch i chng tiu chun thch hp. Ly y dung dch i chng tiu chun v o s hp th bc sng hp th ti a (khong 525 nm). _ Hiu chnh s c bng cch tr i phn hp th ca dung dch nn. V th hiu chun: nh du trn th s c c tng nng tng ng thch hp ca mangan v th. th phi c kim tra mt cch u n theo cc iu kin ti ch v loi ca thit b c s dng. Cch xc nh:

_ Ra ng so mu ca quang k hoc quang ph k trc tin bng dung dch kali permanganat, sau vi nc n nh v sau cng l dung dch th. Sau y dung dch th v o hp th bc sng c dng trong vic chun b th hiu chun. _ Hiu chnh s c bng cch tr i hp th ca dung dch trng c x l tng t. _ Bng th hiu chun, xc nh nng ca mangan tng ng vi tr s hiu chnh v t tnh hm lng mangan ca phn mu th. Biu th kt qu: _ Kt qu l gi tr trung bnh ca kt qu ring bit ca hai ln th nghim. _ Tnh kt qu theo miligam ca mangan trn kilogam ca mu. b. Phng php gii hn Ly khong 10 g mu cao su latex, sy n khi khi lng khng i v ct thnh tng mnh nh. Tro ha mu th: + i vi mu th khng c clo: Ct phn mu th thnh ming nh khng ln hn 0,1 g v cho phn mu th vo mt chn silica 50 ml, t chn vo l trong tm chu nhit, cch nhit. Bt u chun b mt dung dch trng cng mt lc bng cch dng mt cc tng t nhng khng c phn mu th v tip tc x l phn mu th v mu trng trong cng mt phng php ging nhau. Gia nhit chn v mu th bng mt ngn la ga nh cho n khi cn li phn than kh, sau chuyn chn vo l nung c duy tr nhit 550 0C 25 0C v nung cho n khi tt c cacbon b oxy ha. Ly chn ra, lm ngui chn v dng pipet sch thm vo mt lng axit sulfuric m c tng git xung quanh thnh chn lm m u tro. un nh cho n khi ht khi v nung li 550 0C 25 0C t ht cacbon. Lp li cch x l tro bng axit sulfuric m c bng cch thm axit nh trn t mt pipet, un nh cho n khi ht khi vi mc ch gi tro di dng sulfat. chn ngui v thm vo 2 g n 3 g kali hydrogen sulfat v t chn trn tm

chu nhit, cch nhit v un mnh cho n khi phn mu th nu chy tr nn trong sut. Lm ngui chn v mu th. + i vi mu th c clo: _ t mu th trong bnh Kjeldahl, thm 10 ml axit sulfuric v lm nng n khi phn mu th phn hy. Cn thn thm 5 ml axit nitric. Nu phn ng xy ra qu mnh, lm ngui bnh trong cc cha nc lnh v nhit phng t nht l 2 gi trc khi lm nng li. _ Ngay sau khi phn ng u tin xy ra xong, lm nng nh hn hp cho n khi phn ng dng li, sau lm nng mnh hn cho n khi hn hp ha en. Thm 1 ml axit nitric v un nng cho n khi en tr li. Lp li vic thm axit nitric v un nng cho n khi dung dch tr nn mt mu hay vng nht v tr li mu en khi un lu hn. _ Nu s phn hy ko di, cn phi thm 1 ml axit sulfuric trnh cc cht ha cng trong bnh. _ Nu cht phn hy khng c cht khng ha tan, ngui, thm 0,5 ml hydro peroxit v 2 git axit nitric v lm nng cho n khi bc khi. Lp li vic thm hydro peroxit cho n khi khng c s gim mu trong dung dch. Lm ngui pha long bng 10 ml nc v lm nng cho ti khi bc khi. _ Chuyn dung dch v bt k cht cn no cn li vo chn platin dung tch 80 ml, cho bay hi n kh v t chy cho n khi cacbon chy ht. _ Nu cn nhng cht khng tan trong vic phn hy giai on ny, lm ngui, thm vi git axit sulfuric m c v 5 ml axit flohydric. Lm bay hi n kh trn bp ng thi khuy a platin. Lp li thao tc ny hai ln. Nu khng c cht khng ha tan, lm bay hi n kh trn bp. Ha tan mu th: _ Tro thu c qua qu trnh tro ha trn thm 20 ml axit sulfuric pha long v un nng chn trn bp cch thy cho n khi cc cht rn ha tan hay bin mt t thnh chn. Ra cc cht trong chn v cc thy tinh nh, dng a thy tinh to nhng cht rn cha ha tan, un nh dung dch cho n khi tan ht mc. Rt dung dch qua li lc bng thy tinh sch vo mt bnh nn, ra lc v

cht khng tan vi hai hay ba ln nc. Thm vo dung dch trong bnh nn 3 ml axit orthophosphoric, sau cng thm 1 ml kh bt k mu vng no do bi st. _ Thm vo dung dch 0,3 g natri periodat, un si dung dch v duy tr ti im si 10 pht. Gi nhit trn 90 0C thm 10 pht m bo s ln ng mu permanganat. Sau khi lm ngui, bt k s c no do kali periodat ngng t c th lm trong li do ly tm hay lc qua lc li lc bng thy tinh. _ Chuyn dung dch vo mt bnh nh mc dung tch 50 ml v pha ti vch nh mc bng nc n nh 20 0C. Sau khi pha, mu sc phi n nh trong vi gi. Bt k tnh hung phai mu no l do vic loi b khng hon ton tp cht hu c v clorua. Nu iu ny xy ra, lp li vic xc nh nhng dng thm axit sulfuric x l ging nh trong tro ha mu th khng c clo. Chun b cc dung dch i chng tiu chun: _ Chun b mt lot dung dch i chng tiu chun, mi dung dch cha 25 ml nc n nh, 20 ml axit sulfuric v 3 ml axit orthophosphoric. T cc dung dch ny, thm phn dung dch mangan tiu chun thay i t 0 ml (dung dch nn) n 10 ml, cng vi mi trng hp thm 0,3 g natri periodat. un si cc dung dch trong 10 pht m bo ln ng mu. Cui cng, lm ngui v pha long bng nc n nh ti 50 ml trong bnh nh mc. Php o quang ph: _ Ra ng so mu ca quang k hay quang ph k trc tin bng dung dch kali permanganat, sau vi nc n nh v sau cng l dung dch i chng tiu chun thch hp. Ly y dung dch i chng tiu chun v o s hp th bc sng hp th ti a (khong 525 nm). _ Hiu chnh s c bng cch tr i phn hp th ca dung dch nn. V th hiu chun: nh du trn th s c c tng nng tng ng thch hp ca mangan v th. th phi c kim tra mt cch u n theo cc iu kin ti ch v loi ca thit b c s dng. Cch xc nh:

_ Ra ng so mu ca quang k hoc quang ph k trc tin bng dung dch kali permanganat, sau vi nc n nh v sau cng l dung dch th. Sau y dung dch th v o hp th bc sng c dng trong vic chun b th hiu chun. _ Hiu chnh s c bng cch tr i hp th ca dung dch trng c x l tng t. _ Bng th hiu chun, xc nh nng ca mangan tng ng vi tr s hiu chnh v t tnh hm lng mangan ca phn mu th. Biu th kt qu: Kt qu l gi tr trung bnh ca kt qu ring bit ca hai ln th nghim. Tnh kt qu theo miligam ca mangan trn kilogam ca mu.

TI LIU THAM KHO

[1]. S tay phn tch t, nc, phn bn, cy trng ca Vin Th Nhng [2]. TCVN 6319: 2007 [3]. TCVN 6091: 2004 [4]. www.wikidipea.org